Distillation apparatus for recovering citrus essence

ABSTRACT

An aqueous citrus essence is prepared having an enhanced content of components which contribute to the natural flavor of the citrus juice, particularly certain aldehyde type compounds and a decreased content of components, such as easily oxidized fatty substances, which detract from the flavor of the juice. Preparation of the enhanced citrus essence is accomplished by increasing the alcoholic content of the aqueous phase of the essence so that its capacity for desirable aldehyde type components is increased. The increase in alcoholic content is effected by recirculation under appropriate conditions of temperature and pressure of the aqueous phase of the essence in contact with fresh essence. An apparatus is specifically disclosed for effecting the process of the invention. Enhanced essence produced by the present invention is particularly useful for reconstituting the flavor of citrus juice concentrates such as orange juice.

United States Patent [191 Atkins et al.

[451 Jan. 21, 1975 DlSTlLLATlON APPARATUS FOR RECOVERING CITRUS ESSENCE[75] Inventors: Cederic D. Atkins; John A. Attaway,

both of Winter Haven, Fla.

[73] Assignee: State of Florida, Department of Citrus, Lakeland, Fla.

[22] Filed: Sept. 6, 1972 [21] Appl. No.: 286,790

Related U.S. Application Data [62] Division of Ser. No. 109,922, .lanv26, 1971.

Primary ExaminerA. Louis Monacell Assistant Examiner-Frank SeverAttorney, Agent, or FirmJames J. Brown [57] ABSTRACT An aqueous citrusessence is prepared having an enhanced content of components whichcontribute to the natural flavor of the citrus juice, particularlycertain aldehyde type compounds and a decreased content of components,such as easily oxidized fatty substances, which detract from the flavorof the juice. Preparation of the enhanced citrus essence is accomplishedby increasing the alcoholic content of the aqueous phase of the essenceso that its capacity for desirable aldehyde type components isincreased. The increase in alcoholic content is effected byrecirculation under appropriate conditions of temperature and pressureof the aqueous phase of the essence in contact with fresh essence. Anapparatus is specifically disclosed for effecting the process of theinvention. Enhanced essence produced by the present invention isparticularly useful for reconstituting the flavor of citrus juiceconcentrates such as orange juice.

4 Claims, 1 Drawing Figure DISTILLATION APPARATUS FOR RECOVERING CITRUSESSENCE This is a division, of application Ser. No. 109,922, filed Jan.26, 1971.

This application relates to a process and apparatus for recoveringflavor and aroma essences from citrus juices and, more particularly, toa novel process for isolating those essence components which contributeto enhanced odor and flavor in citrus juices without includingundesirable amounts of components normally present in the essence whichcan detract from the odor and flavor of natural juice. This invention isfurther concerned with citrus juice concentrates to which have beenadded specific quantities of the natural flavor and aroma essencesobtained by the process of this invention.

Natural, full strength citrus juices contain a number of essencecomponents which contribute to their flavor and aroma. For example, l2.8Brix orange juice contains about 0.080-0020 percent ethyl alcohol, 0.l0.020 percent peel oil, 0.010-0001 percent various ester components,0.10-0.05 percent fats or fat related compounds, and about 0.001-0.0005percent aldehyde type components.

In order to prepare a concentrate, this juice must be heated to asufficiently high temperature to evaporate some of the water present inthe juice; however, such heating also drives off the various essencecomponents, some of which become entrained in water droplets. Theunfortunate result is that when the resulting juice concentrate isreconstituted (for example, from a 70 Brix concentrate to an about 12Brix juice) by the addition of water, the reconstituted juice has abland taste due to the presence of only traces of remaining oil andwater soluble essence components.

As a result of this problem, it has been the practice to limitconcentrations or orange juice, for example, to no more than about4-fold or 45 Brix (i.e., requiring 3 parts of water to reconstitute 1part of juice concentrate) since, by avoiding additional evaporation ofwater from the natural juice to obtain further concentration, less ofthe essence components are removed.

In addition, it has often been the practice to restore to theconcentrate a portion of the essence components from orange and othercitrus juices removed during concentration of the juice to restore, atleast in part, some of the natural flavor of the juice.

One of the problems which has been associated, however, with the removalof essences from citrus juices is that these essences are composed of anumber of components which effect flavor and aroma of the juice indifferent ways. Further, these components do not always remain presentin the same proportions in the extracted essence as in the naturaljuice. Typically, for example, when orange oil is distilled in thepresence of orangejuice (as in an evaporator unit) there is asignificant decrease in the aldehyde content of the essence and increasein the ester content.

Also, of considerable significance is the fact that some of the essencecomponents either contribute directly to adverse flavor and aroma whenadded back to the juice or undergo chemical changes to form compoundswith undesirable characteristics.

Table 1 gives the composition of essence extracted from 12.8 Brix orangejuice. Table [1 gives the composition of peel oil contained in orangeessence.

TABLE 1 Orange Juice Essence The actual composition of the volatileessence present in citrus juices, and especially orange juice, is quitecomplex and consists of a large number of compounds. For a detailedexamination of these components one may have reference to numerouspublications on the subject. (See Attaway et al, The Isolation andldentification of Some Volatile Carbonyl Components from Orange Juice,Journal of Agricultural Food Chemistry, 10, pp. 102-104; and Attaway etal, Identification of Alcohols and Volatile Organic Acids from NaturalOrange Essence, Journal of Agricultural Food Chemistry, 12, pp. ll8l2l.)

As can be seen in Table 1, however, orange juice essence contains, amongother components, peel oil, consisting largely of d-limonene, fats(including various lipids or fatty esters, e.g., triglycerides) anddiacetyl. This large amount of d-limonene, for example, has been foundto adversely effect flavor and aroma of the essence and to be far inexcess of what is required for reconstitution of the flavor of juices.Further, the lipids present are easily oxidized during heating (as inevaporation and concentration) to components having decidedly unpleasantflavor and aroma characteristics. These undesirable features have alsobeen found to be characteristic of the diacetyl present in the essence.

Of course, present along with these components in the essence are thevarious other compounds which are conveniently grouped as alcohols,esters, and aldehydes (including ketones and diacetyl). Of thesecompounds, the aldehyde type compounds in particular, contributesignificantly to the natural flavor and aroma of the juice. Typical ofthese compounds are n-decanal, geranial, citronellal, ethanol, linalool,n-octanol, terminolene, d-terpineol, and savinene; although it isappreciated that not all of these compounds are, strictly speaking,aldehydes, nor is this an exhaustive list of those components present inorange essence which can be said to enhance the natural orange flavorand aroma.

It is, however, a problem in separating the desirable and undesirableflavor and aroma effecting components of citrus, and especially orangeessences, that the essence readily separates into an aqueous and an oilphase, both of which phases contain desirable essence components. Theoil phase in particular also, however,

contains the greater part of the undesirable flavor components.

Accordingly, because of the mixed presence in the oil and water phase ofthe essence, particularly of both components which contribute to thenatural flavor of the juice and those which either themselves, or intheir oxidation products, adversely effect the flavor and aroma of thejuice, it has been possible to add only limited amounts of theseessences back into either the juice concentrate or the reconstitutedjuice. These amounts have not generally been sufficient, moreover, torestore the natural flavor to the juice.

Thus, in order to more fully restore the natural flavor of concentratedand reconstituted citrus juices, it would be desirable to obtain anessence for reincorporation into the juice which contains selectiveamounts of those components which contribute to the natural flavor andaroma without incorporating those essence components which detract fromthe flavor and aroma.

US. Pat. No. 3,248,233 to Brent et al, for example, describes a processand apparatus for recovering essences from orange juice or other fruitjuice concentrate to enhance the flavor. According to the process of theBrent et al patent, orange juice is first evaporated under vacuum toseparate out the essences which are then contacted with a stream ofwater and subsequently condensed under pressure to obtain a solution ofthe essences. There is, however, no attempt to separate the variouscomponents of the essence according to whether they are features whichenhance or detract from the flavor and aroma of the juicev It is,therefore, an object of the present invention to provide a process andapparatus whereby those components which are present in citrus juiceessence vapors and which contribute to enhanced flavor and odor ofnatural citrus juice are separated and isolated in preselected amountsfrom other components of the es sence vapors which detract from theflavor and odor of natural juice.

It is a further object of this invention to obtain an improved watersoluble essence extract containing desirable flavor, and aromacomponents which can be added to citrus juice which may, for example, bein the form of concentrate, in order to improve the natural flavor andodor of the juice.

These and other objects have been achieved according to the presentinvention, whereby it has been found that desirable flavor and aromaenhancing essence components, which are present in both the oil andaqueous phase of citrus juice essences, can be selectively removed underappropriate conditions from the oil phase into the aqueous phase bycontacting the oil phase with dilute aqueous solutions of alcoholsnaturally occurring in citrus juice essences such as, for example,ethanol. Unexpectedly, it has been found that, under appropriateconditions, the desirable flavor and aroma enhancing components presentin this oil phase are selectively removed into the aqueous alcoholicphase while undesirable components which adversely affect flavor andaroma of orange juice are left behind in the oil phase. Further, sincethe water-soluble phase and the oil phase are mutually immiscible, theoil phase, which is lighter, can readily be separated from the heavierwater phase in to which the alcoholic and flavor and aroma enchancingcomponents have been extracted, resulting in a water soluble essencewhich can be used to reconstruct the natural flavor of citrus juices inreconstituted juices, for example, and which does not contain certaincomponents naturally present in citrus essence but which unfavorablyeffect the flavor of the juice.

In a further embodiment of the present invention, it has been found thatthe level of naturally occurring alcoholic components (primarilyethanol) which are found to be present largely in the aqueous phase ofthe citrus essence, can be greatly and unexpectedly increased up to alevel of up to about percent by repeatedly recirculating and contactingthe water-soluble essence phase as vapor with fresh vaporized orange essences containing both the oil and water-soluble phases. According tothis embodiment of the present invention, the combined water-soluble andoil phases are separated by any convenient method, such as decanting,and the water-soluble phase vaporized and again contacted at appropriateconditions of temperature and pressure with fresh essence vapor toremove alcoholic components from the fresh vapor and further increasethe level of alcoholic components in the watersoluble phase. By carryingout this decanting, vaporization, and re-contacting procedure with thewatersoluble orange essence phase while continually removing excesswater and solid particles from the bottom of a reflux type strippingcolumn and also removing noncondensible vapors and gases from the top ofthe column it is possible to increase the levelof alcoholic componentsin the water soluble phase to about 95 percent.

In yet a further embodiment of the present invention the two proceduresdescribed above are advantageously combined in order to provide a noveltechnique for selectively extracting a water-soluble essence, suitablefor reconstitution into full strength or concentrated orange juice andcontaining selected amounts those flavor and aroma enhancing componentsfound in citrus essence without the presence of excess or undesirableflavor and aroma components such as dlimonene, diaceytyl, and fattyesters and related compounds derived from lipid or fat" constituents oforange juice which are easily oxidized during heating to produceundesirable flavor and aroma components.

According to the present invention, volatile essence vapors are passedinto a reflux type stripping column having heater and condenser sectionswhere pulp, insoluble solids, fatty materials, and excess water areremoved. Air and entrained volatiles (consisting largely of distilledpeel oil, diacetyl, etc.) are removed from the top of the strippingcolumn, while the condensible water and oil essence phases are collectedand removed from the side of the column. In order to properly carry outthis separation as well as subsequent refluxing procedures whereby thealcohol content of the aqueous essence phase is increased, the column ismaintained by a heater at a temperature of about F to 200F and apressure of 24 to 29 inches of mercury.

The combined oil and water essence which is removed from the column isseparated into its respective oil and water phases, for example, bydecanting, the lighter oil phase readily rising to the top of theheavier water phase. The water phase is recycled back into the strippingcolumn and refluxed in contact with additional fresh essence vaporwhereby the level of naturally occurring alcoholic components in thewater phase is increased. Enrichment of the water phase by flavorenhancing aldehyde type components also occurs during the refluxing inthe stripping column. Subsequently, this water phase containing anincreased level of alcoholic components is further contacted with theoil phase and scrubbed with the air and entrained volatile vapors andgases removed previously from the stripping column to further enhanceremoval of aldehydes into the aqueous phase.

This scrubbing procedure removes various ester and aldehyde components(except the esters of formic acid and diacetyl) into the aqueous phasecontaining enhanced alcohol content. Both the aqueous and oil phases arethen removed from the bottom of the scrubber. Non-condensible gases,diacetyl, oxidized fatty compo nents, air, and traces of othercomponents from the combined water and oil phase are conveyed to acondenser where the remaining alcohol, aldehyde, and ester componentsare selectively trapped and combined in desired amounts with the oil andenriched aqueous phase removed earlier from the scrubber. The two phasesbeing mutually immiscible are readily separated and the enriched aqueousessence phase retained. The non-condensed discharge from thecondenser-trip is normally collected for evaluation to determine theextent of removal from the system of the undesirable essence componentscomprising largely diacetyl, fatty vapors, formic acid, and the estersof formic acid. The oil phase which is separated from the aqueousessence phase is largely (about 94-97 percent) d-limonene along withminor amounts of aldehydes, esters, and alcohols.

In the absence of increased amounts of alcohol in the aqueous phasere-circulated to the stripping column for contacting with excess peeloil, the retention of aldehydes is quite low and actually decreases withincreasing concentration of the aqueous essence while the ester contentincreases. Thus, while a l00 fold essence was found to contain 900 ppmof aldehyde and 1,500 ppm esters, when the essence was furtherconcentrated to 300 fold the aldehyde level dropped to 500 ppm and theester level increased to 4,500 ppm, where there was no enrichment ofnatural alcohols present in the aqueous phase.

However, using the techniques of the present invention, whereby thelevel of alcohols present in the aqueous phase was increased to 92percent, and 100 fold essence contained 2,700 ppm aldehydes and 500 ppmesters. Moreover, when the concentration of the aqueous essence phasewas increased to 300 fold, the level of aldehydes was 8,l00 ppm and thelevel of esters was 1,500 ppm.

An additional feature of the present invention is the vacuum control orthe positive air pressure present in the system during essenceconcentration. A vacuum lower than 24 inches of mercury providessufficient oxygen to initiate the oxidation of ethyl alcohol andassociated components to yield artifacts of aldehyde and ester nature inconsiderable quantity. This results in definite changes in thealcohol-aldehyde ratio present in the folded essences. Excessiverecycling in the stripping column produces an equivalent effect andshould be avoided. Thus the production of relatively anhydrous essencesare more representative of fresh citrus juice essences when manufacturedat a vacuum in excess of 24 inches, preferably about 2429 inches ofmercury. During production of high-fold relatively anhydrous essencescondenser temperatures are most effective for prevention of losses at32F or below.

For a further understanding of the present invention, reference is nowmade to the Figure which shows an essence recovery unit for selectivelyrecovering citrus essence containing components having desirable flavorand aroma properties but which are substantially free of deleteriouscomponents such as excess d-limonene, diacetyl, and lipids which areeasily oxidized to produce unpleasant flavor and odor.

A spiral stripping column is shown generally at l, which is providedwith a boiler 7 located at the bottom of the column with dischargeoutlets located at the lower portion at 17 and 18. An overhead condenser2 is located atop the spiral stripping column with a vent 8 at the topand inlets and outlets at 12 and 10 respectively. A trap for separatingthe water soluble and oil components of the essence is shown at 3. Acondensercooler is shown at 4 for cooling non-condensible vapors andgases in one stream and the oil phase from the trap in another separatestream. Cooling for the condenser 4 is provided by suitablerefrigeration supplied externally but not shown. A scrubber is shown at5 for counter-currently contacting the oil phase and alcohol enrichedwater soluble phase along with non-condensible vapors and gases. Thecondenser 6 which contains a number of plates provides for condensingand removal of further oil essence from the gaseous residues from thescrubber 5. The decant vessel shown at 16 where the aqueous and oilphases from the scrubber 5 and condenser 6 are combined and thenseparated into their oil and water soluble components. The heavier watersoluble phase containing alcoholic components and flavor and aromaenhancing constituents which have been removed in the scrubber 5 areremoved from the bottom of the decant flavor and passed to suitablestorage tank shown at 19. From this storage tank the water solubleessence containing the desired components can be removed and used toenhance the flavor of reconstituted orange juice etc. as desired.

According to the process of the instant invention, orange essence vaporsof about to 300 fold, which contain less than about 0.08 percent oiland, for example, which can be obtained by conventional procedures suchas flash evaporation of extracted juice under vacuum, are passed at atemperature of about l40200F at 20 into the spiral stripping column 1,having a boiler at the lower end shown at 7 which maintains thestripping column at a sufficient temperature to keep the essencevaporized. Various components such as fat bearing insoluble particlesalong with water are separated from the essence vapors at bottoms at 17and 18 while non-condensible vapors and traces of components passupwards in the column 1 and out of the top of the condenser at 8.Removal of these non-condensible vapors is facilitated by use of avacuum of about 24-29 inches of mercury. Condensibles, which includeboth the oil and water-soluble phases are condensed in the overheadcondenser 2 and flow back downward into the stripping column until theyreach the collecting plate shown at 9 where they collect and flow out ofthe condenser at 10 to the trap shown at 3. In the trap, the heavierwater soluble components collect at the bottom whereas the lighter oilphase collects at the top. Thus, the water phase can be removed at theside bottom of the trap 11 and returned to the spiral stripping columnat 12 and overhead condenser for additional refluxing and contactingwith fresh essence vapors, or alternatively, as desired, removed throughthe bottom of the trap 13. The lighter oil phase is removed from thetrap through the top side opening 14 and then passed to one side of thecooler shown at 4.

As previously discussed, recycling of the water phase from the bottomside 11 of the trap 2 back into the spiral stripping column where it isrefluxed with fresh essence vapor, has been found by the practice ofthis invention to result in increased levels of naturally occurringalcohol content in the water-soluble phase up to about 95 percent in thevapor present in the overhead condenser and also to increase the removalof aldehyde components into the aqueous phase. The water soluble phasecontaining the desired amount of alcoholic components and enhancedcontent of aldehyde type compounds is removed from the bottom of thetrap 13 and directed at 15 into the stream of condensed oil phase fromthe top side of the trap 14 and condenser 4 and the mixture of the twocomponents then passed into the scrubber 5 where the mixture iscontacted at a temperature of about 4560F with the non-condensible gaseswhich have been taken from the top of the overhead condenser 8, andpassed through the cooling condenser 4 in a separate stream from the oilphase coming from the trap 2. In the scrubber 5, the water-soluble phasecontaining the enhanced level of alcoholic content selectively stripsaway additional desirable aldehyde type components from the oil phaseand then is passed together with the oil phase out of the scrubber 5 tothe decant vessel 16.

Undesirable components comprising primarily noncondensible fattyelements as well as traces of peel oil and other essence components aredirected out of the scrubber 5 at the top to the condenser unit 6 whichcontains a number of reflux shelves and is maintained at a temperatureof about 3240F, By controlling the number of shelves or plates in thecondenser the quantity of essence components and non-condensible vaporcomponents recovered from the condenser 6 is determined. The moreshelves present in the condenser, the greater will be the quantity ofretained components of this type which are directed out of the bottom 21of the condenser 6 to the decant vessel 16 where they are combined withthe oil and water-soluble components from the scrubber 5. Typically,about 6-12 shelves are advantageously employed in the condenser.Generally, however, it is desirable to limit the amount of thesecomponents to not more than about 0.2 percent of the total fattymaterial present. Components such as the highly volatile diacetyl whichare not removed from the condenser at 21 and conveyed to the decantvessel 16 are removed from the top of the condenser at 22 for analysisor discarded. Removal of these residual components is facilitated byapplication of a vacuum.

Condensed liquid comprising both the water-soluble phase and oil phaseis removedfrom the bottom of the scrubber 5 at 23 and combined in thedecant vessel 16 with the recovered components from the condenser 6. Inthe decant vessel, which is maintained at a temperature of about 3540Fthe oil and water phase are separated with the lighter oil phase beingon top and the water-soluble phase removed through a tap at the bottomof the decanter vessel. This water soluble phase, which contains thedesirable flavor and aroma components is then stored in a tank 19preferablyprovided with means for chilling.

As previously pointed out, the percentage of alcohol present in themixture presented into the scrubber 5 determines the quantity ofaldehydes and certain other flavor components removed from the oil phaseand retained in the water phase during contacting with fresh essence inthe stripping column and during scrubbing with the non-condensible ventgases. Moreover, if the concentration of alcoholic water-soluble essenceis carried to about percent, the alcohol (plus very little water) andthe oil phase are entirely miscible. Such high alcohol levels aregenerally not desirable, however, since the entire oil phase is therebyextracted resulting in the inclusion of a high level of undesirablecomponents (e.g., d-limonene). Generally, however, these high alcoholconcentrations are encountered in the vapor present in the overheadcondenser atop the stripping column. Condensation produces substantialdilution of the alcoholic components as well as extracted flavorcomponents. Further, some state regulations do not permit the inclusionof greater than 0.03 percent by volume of oil into single strengthorange juice or concentrate so that the level of oil extracted into thewater phase should be kept relatively low.

Advantageously, the aqueous phase obtained by the process of thisinvention contains about l070, preferably about 60 percent naturalalcoholic components (mostly ethanol). At this range of alcohol levelextractions of about 2,500 to 9,000 ppm of aldehyde and ketone typecomponents which contribute to improved flavor and aroma are obtainedwhile levels of fatty acids or esters or their oxidation products aremaintained below about 10 ppm. Most advantageously, the level of thesecomponents in the final water-soluble extract is about 3,0004,500 ppm.At alcohol levels of below 5 percent only a level of 1,500 ppm aldehydeand ketone components is realized.

As heretofore noted, it is commonly the practice to separate citrusessence (e.g., by flash evaporation) from the fresh juice prior toconcentration of the juice. In this manner, oxidation of the fattycomponents present in the essence is to a degree limited since theremoved essence is not then subject to heating required to concentratethe juice to the desired Brix. The concentrate obtained in this way,however, is somewhat bland and requires reconstitution with a portion ofthe removed essence. Since this essence, however, contains fattycompounds which are nevertheless oxidized to a degree sufficient toadversely affect odor and taste, it is impossible to completely restorethe natural flavor and aroma of the juice. This problem become moreacute as higher degrees of concentration are reached in the juice, sinceproportionately more of the extracted essence must be added back to theconcentrate to restore a semblance of the original flavor and aroma orreconstitution of the juice. Present orange juice concentrate,therefore, are limited to about 4 fold or 4550 Brix.

Using the essence prepared by the instant invention, however, whichcontains not more than about 0.2 percent total fatty materials, juiceconcentrates of substantially higher Brix can be prepared which onreconstitution to the single strength juice of about 12.5 Brix, havepresent essentially the same amounts of naturally occurring aldehydes,ketones, alcohols, and oil which contribute to flavor and aroma as theoriginal single strength juice substantially without the fattycomponents which adversely affect the flavor and aroma.

Generally, the water-soluble essence prepared according to the presentinvention can have the composi- TABLE IV Water-Soluble Essence ComponentPercent (by vol.)

Alcohols 4 2 Aldehydes 0.27-0.71 Esters 0.05-0.15 Oil 0020-0080 (mostlyd-limonene) Table V gives the composition of the oil phase from whichthe water-soluble Essence of Table IV is separated.

TABLE V Oil Phase Component Percent (by vol.)

d-limonene 94-97 Aldehydes 0.93-4.60 Esters 0.04-1.50 Alcohols 1.0 20

Table V1 gives the composition of actual aqueous essences prepared bythe present invention.

TABLE VI Water-soluble essence derived from 100 gallons of orange juiceof 12.8 Brix or 12.8% sugar solids Compressed to the indicated gallonsof essence Corresp. Vac. 24.04 in Hg.

(21) 1 gal. 40 40,000 ppm alcohol (ethyl) 100 fold 0.27 2,700 ppmaldehydes essence 0.05 500 ppm esters (b) gal. 8.0 80,000 ppm alcohol(ethyl) 200 fold 0.54 5,400 ppm aldehydes essence 0.10 1,000 ppm esters(c) Vs gal. 12.0 120,000 ppm alcohol (ethyl) 300 fold 0.71 8,100 ppmaldehydes essence 0.15 1,500 ppm esters Depending, among other things,on the degree of concentration of the juice, the water-soluble essenceof this invention can be prepared to the desired concentration (fold),aldehyde, ketone, alcohol, and oil content. The following Table Vllgives examples of typical orange essences prepared by the instantinvention and used to restore the natural flavor etc. of high Brixconcentrate:

containing 4000 ppm aldehyde, ketone, and alcohol; about 0.2% totall'atty material 200 ppm water soluble essence. 0.020% peel oil byvolume.

Table VllContinued Essence Strength Pump-out Before Reconstituted (Foldbased on strength of Reconstitution concentrate essence in singlestrength with essence fresh juice) 3 200 fold essence 65 Brix 62 Brixcontaining 4000 ppm 250 ppm water aldehyde, ketone, and soluble essence.alcohol; about 0.2% 0.020% peel oil total fatty material by volume.

4v 300 fold essence 65 Brix 56.6 Brix containing 6000 ppm 200 ppm wateraldehyde, ketone, and soluble essencev alcohol; about 0.2% 0.020% peeloil total fatty material by volume.

The preferred high density concentrates of the present invention areabout 5 to 6 fold concentrates of about 55 to 65 Brix and havingviscosities not exceeding about 5,000 cp at F and preferably about200-4,000 c. The level of water soluble essence (aldehydes, ketones, andalcohols) present is preferably about 150-400 ppm in the reconstitutedconcentrates and most preferably about 200300 ppm.

EXAMPLE 1 Essence vapors obtained from extracted orange juice by flashevaporation were passed into a spiral stripping column at a temperatureof about [40F and a rate of 1,000 lbs/hr. The spiral stripping columnwas provided with a heating unit at its base and an overhead refluxcondenser. During the continuous refluxing of the essence vapors at atemperature of 140F, water and solid fruit particles including fatbearing insolubles were removed from the bottom of the stripping columnwhile non-condensible vapors and gases were removed from the top of theoverhead condenser with the aid of a vacuum of 24 inches of Hg. Watersoluble essence oils were collected near the bottom of the overheadcondenser and passed to a trap where the heavier water solublecomponents were separated from the oil phase. The water solublecomponents were continuously recycled back into the overhead portion ofthe stripping column and the alcoholic content of the water solublephase forming the bottom layer in the trap monitored and water solubleessence withdrawn as it reached a level of 15 percent by volume totalalcohols. Simultaneously, the oil phase forming the top layer in thetrap was drawn off at a rate of 4 gal./hr. and then passed along withthe water soluble phase into a scrubber where the non-condensible gasesand vapors from the overhead condenser were passed in counter-currentflow to these combined liquids at a temperature of 45F. Residual gaseswere removed from the top of the scrubber and combined oil and watersoluble liquid withdrawn from the bottom of the scrubber and decanted ata temperature of about 45F. At the same time the non-condensible gasesremoved from the top of the scrubber were passed to a trap containingplates where additional oily components were condensed out. Thesecondensed components were then combined at a rate of 0.5 gal/hr. withthe liquid discharge from the bottom of the scrubber in a decantingvessel at a temperature of 45F and the water soluble phase from thebottom layer in the decant vessel removed and stored in a chilled tank.Analysis of the fold water soluble essence removed from the decantvessel showed it to be 4.2 percent alcohol, 0.32 percent combinedketones and aldehydes, 0.050 percent oil and 0.005 percent fattymaterials.

What is claimed is:

1. An apparatus for preparing citrus essence which comprises a verticalstripping column with overhead reflux condenser means disposed atop saidcolumn for returning condensibles to said stripping column andseparating non-condensibles therefrom; said condenser means having anexit port means in the upper portion of said condenser for removing saidnon-condensibles, heater means disposed at the lower portion of thecolumn, liquid collecting plate means located at the base of saidcondenser means and within said stripping column and side port forintroducing citrus essence vapor; means for separating liquids ofdifferent densities operatively connected to receive and separatecondensed liquids collected and removed from said liquid collectingmeans disposed at the base of said overhead condenser and meansconnecting to said separation means for continuously returning the moredense of said liquids to said stripping column at a point below thepoint at which condensed liquids are removed from the stripping column;a conduit operatively connected to an exit port in the upper portion ofsaid overhead condenser for removing non-condensable vapors from saidcondenser and an exit port at the bottom of said stripping column forremoving bottoms; scrubber means for contacting both the more dense andless dense liquids removed from said separator means with saidnoncondensable vapors from the overhead condenser, said scrubber meansbeing operatively connected to an exit port means in the bottom of saidseparator means for removing said more dense liquid and by a conduitmeans in the upper portion of the separator means for removing the lessdense liquid contained therein,

whereby said less dense and said more dense liquids are introduced intothe top of said scrubber and said noncondensable gas are introduced tothe bottom of said scrubber whereby a countercurrent scrubbing of saidnon-condensable gases is effected by said downward passing liquids; thescrubber also being provided with an exit port at its bottom portion forremoving said liquids to a separating tank and an overhead exit port forremoving upward flowing gases; said overhead exit port in said scrubberbeing further connected to the top of second condenser means forremoving liquids entrained in said non-condensable gases; said secondcondenser means also having an exit port at its bottom for removing saidentrained condensed liquids and a second overhead exit port for removinggases; the exit port at the bottom of the condenser being connected tothe separating tank, and collection means connected with said separatingtank.

2. The apparatus of claim 1 which further includes vacuum producingmeans operatively connected to said overhead exit port on said secondcondenser means for maintaining a vacuum in said system and removingnon-condensed gases.

3. The apparatus of claim 1 which further includes refrigeration meansoperatively disposed for cooling said non-condensable gases from theoverhead exit port in said first condenser and for cooling said lessdense liuqid removed from said separator means.

4. The apparatus of claim 1 wherein said condenser means is providedwith from 6 to 12 horizontal, separated vertically, disposed plates tofacilitate the selective condensation of liquids.

1. AN APPARATUS FOR PREPARING CITRUS ESSENCE WHICH COMPRISES A VERTICALSTRIPPING COLUMN WITH OVERHEAD REFLUX CONDENSER MEANS DISPOSED ATOP SAIDCOLUMN FOR RETURNING CONDENSIBLES TO SAID STRIPPING COLUMN ANDSEPARATING NONCONDENSIBLES THEREFROM; SAID CONDENSER MEANS HAVING ANEXIT PORT MEANS IN THE UPPER PORTION OF SAID CONDENSER FOR REMOVING SAIDNON-CONDENSIBLES, HEATER MEANS DISPOSED AT THE LOWER PORTION OF THECOLUMN, LIQUID COLLECTING PLATE MEANS LOCATED AT THE BASE OF SAIDCONDENSER MEANS AND WITHIN SAID STRIPPING COLUMN AND SIDE PORT FORINTRODUCING CITRUS ESSENCE VAPOR; MEANS FOR SEPARATING LIQUIDS OFDIFFERENT DENSITIES OPERATIVELY CONNECTED TO RECEIVE AND SEPARATECONDENSED LIQUIDS COLLECTED AND REMOVED FROM SAID LIQUID COLLECTINGMEANS DISPOSED AT THE BASE OF SAID OVERHEAD CONDENSER AND MEANSCONNECTING TO SAID SEPARATION MEANS FOR CONTINUOUSLY RETURNING THE MOREDENSE OF SAID LIQUIDS TO SAID STRIPPING COLUMN AT A POINT BELOW THEPOINT AT WHICH CONDENSED LIQUIDS ARE REMOVED FROM THE STRIPPING COLUMN;A CONDUIT OPERATIVELY CONNECTED TO AN EXIT PORT IN THE UPPER PORTION OFSAID OVERHEAD CONDENSER FOR REMOVING NON-CONDENSABLE VAPORS FROM SAIDCONDENSER AND AN EXIT PORT AT THE BOTTOM OF SAID STRIPPING COLUMN FORREMOVING BOTTOMS; SCRUBBER MEANS FOR CONTACTING BOTH THE MORE DENSE ANDLESS DENSE LIQUIDS REMOVED FROM SAID SEPARATOR MEANS WITH SAIDNON-CONDENSABLE VAPORS FROM THE OVERHEAD CONDENSER, SAID SCRUBBER MEANSBEING OPERATIVELY CONNECTED TO AN EXIT PORT MEANS IN THE BOTTOM OF SAIDSEPARATOR MEANS FOR REMOVING SAID MORE DENSE LIQUID AND BY A CONDUITMEANS IN THE UPPER PORTION OF THE SEPARATOR MEANS FOR REMOVING THE LESSDENSE LIQUID CONTAINED THEREIN, WHEREBY SAID LESS DENSE AND SAID MOREDENSE LIQUIDS ARE INTRODUCED INTO THE TOP OF SAID SCRUBBER AND SAIDNON-CONDENSABLE GAS ARE INTRODUCED TO THE BOTTOM OF SAID SCRUBBERWHEREBY A COUNTERCURRENT SCRUBBING OF SAID NONCONDENSABLE GASES ISEFFECTED BY SAID DOWNWARD PASSING LIQUIDS; THE SCRUBBER ALSO BEINGPROVIDED WITH AN EXIT PORT AT ITS BOTTOM PORTION FOR REMOVING SAIDLIQUIDS TO A SEPARATING TANK AND AN OVERHEAD EXIT PORT FOR REMOVINGUPWARD FLOWING GASES; SAID OVERHEAD EXIT PORT IN SAID SCRUBBER BEINGFURTHER CONNECTED TO THE TOP OF SECOND CONDENSER MEANS FOR REMOVINGLIQUIDS ENTRAINED IN SAID NON-CONDENSABLE GASES; SAID SECOND CONDENSERMEANS ALSO HAVING AN EXIT PORT AT ITS BOTTOM FOR REMOVING SAID ENTRAINEDCONDENSED LIQUIDS AND S SECOND OVERHEAD EXIT PORT FOR REMOVING GASES;THE EXIT PORT AT THE BOTTOM OF THE CONDENSER BEING CONNECTED TO THESEPARATING TANK, AND COLLECTION MEANS CONNECTED WITH SAID SEPARATINGTANK.
 2. The apparatus of claim 1 which further includes vacuumproducing means operatively connected to said overhead exit port on saidsecond condenser means for maintaining a vacuum in said system andremoving non-condensed gases.
 3. The apparatus of claim 1 which furtherincludes refrigeration means operatively disposed for cooling saidnon-condensable gases from the overhead exit port in said firstcondenser and for cooling said less dense liuqid removed from saidseparator means.
 4. The apparatus of claim 1 wherein said condensermeans is provided with from 6 to 12 horizontal, separated vertically,disposed plates to facilitate the selective condensation of liquids.